Acta Crystallographica. Section C, Structural Chemistry

Reports of quadrivalent transition-metal fluoride salts containing bulky organic cations are limited. In this context, we prepared the bis(tetraphenylarsonium) hexafluoridotechnetate(IV) dihydrate salt, (C24 H20 As)2 [TcF6 ]·2H2 O, by a cation metathesis reaction of (NH4 )2 [TcF6 ] in water. This is the first report of an arsonium salt of the hexafluoridotechnetate(IV) dianion. (AsPh4 )2 [TcF6 ]·2H2 O crystallizes in the triclinic space group P-1. The [TcF6 ]2- anion adopts a slightly distorted octahedral geometry with an average Tc-F bond length of 1...

A high-pressure phase of magnesium chloride hexahydrate (MgCl2 ·6H2 O-II) and its deuterated counterpart (MgCl2 ·6D2 O-II) have been identified for the first time by in-situ single-crystal X-ray and powder neutron diffraction. The crystal structure was analyzed by the Rietveld method for the neutron diffraction pattern based on the initial structure determined by single-crystal X-ray diffraction. This high-pressure phase has a similar framework to that in the known ambient-pressure phase, but exhibits some structural changes with symmetry reduction caused by a subtle modification in the hydrogen-bond network around the Mg(H2 O)6 octahedra...

A novel hydrolytic stable CoII -organic framework, namely poly[[bis(2-amino-4-sulfonatobenzoato-κO1 )tetraaquatris{μ-1,4-bis[(imidazol-1-yl)methyl]benzene-κ2 N3 :N3' }dicobalt(II)] tetrahydrate], {[Co(C7 H5 NO5 S)(C14 H14 N4 )1.5 (H2 O)2 ]·2H2 O}n , (1), based on multifunctional 2-amino-5-sulfobenzoic acid (H2 asba) and the auxiliary flexible ligand 1,4-bis[(imidazol-1-yl)methyl]benzene (bix), was prepared using the solution evaporation method. The purity of (1) was confirmed by elemental analysis and powder X-ray diffraction (PXRD) analysis...

Three novel coordination polymers (CPs), namely poly[[di-μ-aqua-bis{μ4 -3,3'-[(5-carboxylato-1,3-phenylene)bis(oxy)]dibenzoato-κ5 O1 :O1' ,O3 :O5 :O5' }bis(1,10-phenanthroline-κ2 N,N')trinickel(II)] dimethylformamide 1.5-solvate trihydrate], {[Ni3 (C21 H11 O8 )2 (C12 H8 N2 )2 (H2 O)2 ]·1.5C3 H7 NO·3H2 O}n , (I), poly[[di-μ-aqua-bis{μ4 -3,3'-[(5-carboxylato-1,3-phenylene)bis(oxy)]dibenzoato-κ5 O1 :O1' ,O3 :O5 :O5' }bis(1,10-phenanthroline-κ2 N,N')tricobalt(II)] diethylamine disolvate tetrahydrate], {[Co3 (C21 H11 O8 )2 (C12 H8 N2 )2 (H2 O)2 ]·2C2 H7 N·4H2 O}n , (II), and catena-poly[[aqua(1,10-phenanthroline-κ2 N,N')zinc(II)]-μ-5-(3-carboxyphenoxy)-3,3'-oxydibenzoato-κ2 O1 :O3 ], [Zn(C21 H12 O8 )(C12 H8 N2 )(H2 O)]n , (III), have been synthesized by the reaction of different metal ions (Ni2+ , Co2+ and Zn2+ ), 3,3'-[(5-carboxy-1,3-phenylbis(oxy)]dibenzoic acid (H3 cpboda) and 1,10-phenanthroline (phen) under solvothermal conditions...

Thermal analysis, X-ray diffraction and temperature-dependent IR spectroscopy were used to study the dehydration process of crystalline DL-phenylglycinium trifluoromethanesulfonate monohydrate (PGTFH), C8 H10 NO2 + ·CF3 SO3 - ·H2 O. PGTFH dehydrates in one step centred at 353 K and crystallizes in the monoclinic space group C2/c, whereas the anhydrous compound (PGTF) crystallizes in the triclinic space group P-1. The dehydration process in PGTFH is preceded by a weakening of both the noncovalent aromatic-aromatic interactions and the packing contacts...

Coordination polymers (CPs) have attracted increasing interest in recent years. In this work, two new CPs, namely poly[[aquabis(2,2'-bipyridine-κ2 N,N'){μ3 -5-[(4-carboxylatophenoxy)methyl]benzene-1,3-dicarboxylato-κ4 O1 ,O1' :O3 :O5 }(μ-formato-κ3 O:O,O')dicadmium(II)] monohydrate], {[Cd2 (C16 H9 O7 )(HCO2 )(C10 H8 N2 )2 (H2 O)]·H2 O}n (1), and poly[[(2,2'-bipyridine-κ2 N,N'){μ3 -5-[(4-carboxylphenoxy)methyl]benzene-1,3-dicarboxylato-κ4 O1 ,O1' :O3 :O5 }manganese(II)] sesquihydrate], {[Mn(C16 H10 O7 )(C10 H8 N2 )]·1...

The three organic two-photon-absorbing cycloalkanone chromophores 2,4-bis[4-(diethylamino)benzylidene]cyclobutanone, C26 H32 N2 O (I), 2,5-bis[4-(diethylamino)benzylidene]cyclopentanone, C27 H34 N2 O (II), and 2,6-bis[4-(diethylamino)benzylidene]cyclohexanone, C28 H36 N2 O (III), were obtained by a reaction between 4-(diethylamino)benzaldehyde and the corresponding cycloalkanone and were characterized by single-crystal X-ray diffraction studies, as well as density functional theory (DFT) quantum-chemical calculations...

This study of 3-(5-phenyl-1,3,4-oxadiazol-2-yl)-2H-chromen-2-one, C17 H10 N2 O3 , 1, and 3-[5-(pyridin-4-yl)-1,3,4-oxadiazol-2-yl]-2H-chromen-2-one, C16 H9 N3 O3 , 2, was performed on the assumption of the potential anticancer activity of the compounds. Three polymorphic structures for 1 and two polymorphic structures for 2 have been studied thoroughly. The strongest intermolecular interaction is stacking of the `head-to-head' type in all the studied crystals. The polymorphic structures of 1 differ with respect to the intermolecular interactions between stacked columns...

Exploratory studies in the systems A-Al-Sn (A = K and Rb) yielded the clathrates K8 Alx Sn46-x (potassium aluminium stannide) and Rb8 Alx Sn46-x (rubidium aluminium stannide), both with the cubic type-I structure (space group Pm-3n, No. 223; a ≃ 12.0 Å). The Al:Sn ratio is close to the idealized A8 Al8 Sn38 composition and it is shown that it can be varied slightly, in the range of ca ±1.5, depending on the experimental conditions. Both the (Sn,Al)20 and the (Sn,Al)24 cages in the structure are fully occupied by the guest alkali metal atoms, i...

Single crystals of two new bimetallic oxalate compounds with the formula [ACr(C2 O4 )2 (H2 O)4 ]n (A = Li or Na), namely catena-poly[[diaqualithium(I)]-μ-oxalato-κ4 O1 ,O2 :O1' ,O2' -[diaquachromium(III)]-μ-oxalato-κ4 O1 ,O2 :O1' ,O2' ], (I), and catena-poly[[diaquasodium(I)]-μ-oxalato-κ4 O1 ,O2 :O1' ,O2' -[di-aquachromium(III)]-μ-oxalato-κ4 O1 ,O2 :O1' ,O2' ], (II), have been synthesized, characterized and their crystal structures elucidated by X-ray diffraction analysis and compared. The compounds crystallize in the monoclinic space group C2/m for (I) and in the triclinic space group P-1 for (II); however, they have somewhat similar features...

The cyanide ligand can act as a strong σ-donor and an effective π-electron acceptor that exhibits versatile bridging abilities, such as terminal, μ2 -C:N, μ3 -C:C:N and μ4 -C:C:N:N modes. These ligands play a key role in the formation of various copper(I) cyanide systems, including one-dimensional (1D) chains, two-dimensional (2D) layers and three-dimensional (3D) frameworks. According to the literature, numerous coordination polymers based on terminal, μ2 -C:N and μ3 -C,C,N bridging modes have been documented so far...

Reported in this contribution are the synthesis and crystal structures of two new FeIII complexes of 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane (HMC), namely, dichlorido(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)iron(III) chloride, [FeCl2 (C16 H36 N4 )]Cl or cis-[FeCl2 (rac-HMC)]Cl (1), and dichlorido(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)iron(III) tetrachloridoferrate, [FeCl2 (C16 H36 N4 )][FeCl4 ] or trans-[FeCl2 (meso-HMC)][FeCl4 ] (2). Single-crystal X-ray diffraction studies revealed that both 1 and 2 adopt a pseudo-octahedral geometry, where the macrocycles adopt folded and planar geometries, respectively...

Two organic-inorganic hybrid layered materials, namely poly[(μ-1,4-diaminobenzene-κ2 N:N')[μ3 -sulfato(VI)-κ4 O:O':O'',O''']manganese], [Mn(SO4 )(C6 H8 N2 )]n , 1, and poly[(μ-1,4-diaminobenzene-κ2 N:N')[μ3 -sulfato(VI)-κ4 O:O':O'',O''']copper], [Cu(SO4 )(C6 H8 N2 )]n , 2, have been synthesized using 1,4-phenylenediamine (PPD) as an organic template and component (linker). Both materials form three-dimensional frameworks. The crystal structures were determined using data from powder X-ray diffraction measurements...

A new potassium dysprosium polyborate, K3 DyB6 O12 , has been prepared via the high-temperature molten salt method and structurally characterized by single-crystal X-ray diffraction analysis. The structure can be described as a three-dimensional framework composed of isolated bicyclic [B5 O10 ]5- groups and Dy3+ and K+ ions. The Fourier transform IR (FT-IR) and ultraviolet-visible (UV-Vis) spectra were investigated. A series of K3 Gd1-x Dyx B6 O12 phosphors was prepared and their photoluminescence properties were studied...

The first ternary BaF2 -Ln(Y)F3 -ZrF4 phases crystallizing near the composition range of fluoride glasses, namely Ba4 YZr3 F23 (barium yttrium fluoridozirconate) and isotypic Ba4 LnZr3 F23 (Ln = Yb, Er and Nd), have been synthesized. The crystal structure of Ba4 YZr3 F23 cannot be correctly determined in the centrosymmetric space group Pnma (R1 = 0.09); it is preferably described in the noncentrosymmetric space group Pn21 a (R1 = 0.028). All cations are located at y = 0.25-0.29 and 0.75-0.79. This new structure type is formed by infinite {[YZr3 F23 ]8- }n columns associating, along [001], YF9 tricapped trigonal prisms, ZrF8 dodecahedra and ZrF7 polyhedra...

The low-temperature triclinic variety α-BaZr2 F10 constitutes a new structure type, less symmetrical than the higher-temperature β-variety. It is based on the stacking of double sheets of Zr polyhedra, connecting three different kinds of ZrF7 polyhedra and one ZrF8 polyhedron via vertices and edges, separated by corrugated Ba2+ layers. It is compared to the high-temperature β-variety, directly recrystallizing from barium fluoridozirconate glass, and also to BaTe2 F10 and KTe2 F9 .

A new cyanide-bridged FeIII -MnII heterobimetallic coordination polymer (CP), namely catena-poly[[[N,N'-(1,2-phenylene)bis(pyridine-2-carboxamidato)-κ4 N,N',N'',N''']iron(III)]-μ-cyanido-κ2 C:N-[bis(4,4'-bipyridine-κN)bis(methanol-κO)manganese(II)]-μ-cyanido-κ2 N:C], {[FeMn(C18 H12 N4 O2 )(CN)2 (C10 H8 N2 )2 (CH3 OH)2 ]ClO4 }n , (1), was prepared by the self-assembly of the trans-dicyanidoiron(III)-containing building block [Fe(bpb)(CN)2 ]- [bpb2- = N,N'-(1,2-phenylene)bis(pyridine-2-carboxamidate)], [Mn(ClO4 )2 ]·6H2 O and 4,4'-bipyridine, and was structurally characterized by elemental analysis, IR spectroscopy, single-crystal X-ray crystallography and powder X-ray diffraction (PXRD)...

A second polymorph of phenylselenium trichloride, PhSeCl3 or C6 H5 Cl3 Se, is disclosed, which is comprised of asymmetric chlorine-bridged noncovalent dimer units rather than polymeric chains. These dimers are each weakly bound to an adjacent dimer through noncovalent Se...Cl bonding interactions. Phenyl rings within each dimer are oriented in a syn fashion. Density functional theory (DFT) calculations reveal that the putative anti isomer is within 5 kJ mol-1 of the experimentally observed form. This structure represents the first additional polymorph discovered for an organoselenium trihalide compound...

We report the crystal structure and crystallization conditions of a first hydrated form of metacetamol (a hemihydrate), C8 H9 NO2 ·0.5H2 O. It crystallizes from metacetamol-saturated 1:1 (v/v) water-ethanol solutions in a monoclinic structure (space group P21 /n) and contains eight metacetamol and four water molecules per unit cell. The conformations of the molecules are the same as in polymorph II of metacetamol, which ensures the formation of hydrogen-bonded dimers and R2 2 (16) ring motifs in its crystal structure similar to those in polymorph II...

The title compound, C37 H42 , is a new mesogenic compound containing the fluorene moiety. It exhibits enantiotropic nematic liquid crystalline behaviour with melting at 125 °C and isotropization at 175 °C. The crystallographically independent unit contains two molecules oriented face-to-edge with respect to each other. The two molecules have nearly the same conformation of the bis-phenyl fluorene moiety. The molecular packing in the crystal phase is nematic-like.